Experiment 15:

Quality Control for the Athenium Baking Soda Company Lab Report

Katrina Le

Kaitlynn Jackson

Lab Section 201

Wednesday, January 25, 2017

Introduction

Baking soda is a common name for sodium hydrogen carbonate or N aHCO 3 (s) . It is a

useful compound that can be found in many everyday products. The Athenium Baking Soda

Company recently started producing baking soda using a method that reacts crystalline

ammonium hydrogen carbonate with brine, which contains high concentrations of sodium

chloride as well as traces of potassium chloride, lithium chloride, and calcium chloride that may

be present in the dry residue. Because of this, the Athenium Baking Soda Company wants to

hire quality control scientists to test for contaminants in their baking soda. To do this, the

Athenium Baking Soda Company has decided that applicants compete to analyze the

composition and purity of baking soda samples. The purpose of this experiment is to analyze the

composition of the baking soda using two different methods to figure out the percentage of

N aHCO 3 in the baking soda and by determining the impurities present in the sample.

This experiment will enable our team to use what we learned in the Thermal Gravimetric

Analysis Lab (Experiment 4), Emission Analysis of Aqueous Solutions of Groups IA and IIA

Metal Salts Lab (Experiment 10), and Determination of the Concentration of Acetic Acid in

Vinegar Lab (Experiment 12). The methods learned in these previous experiments will be used

except with different reagents. By combining the methods learned into one experiment, the

experiment reinforces knowledge as well as provides a better understanding of chemistry as a

science.

The baking soda will be analyzed for metal ion contaminants with a MeasureNet

spectrophotometer using emission spectroscopy. Spectroscopy is best explained as a measure of

molecular energy levels which are most commonly expressed in the form of emissions or
absorptions. Because each of the metal ion contaminants releases certain wavelengths of light,

the emission spectra of the baking soda can be graphed along with the emission spectra for K + ,

Li+ , and C a2+ using standard 0.1 M solutions for each with the spectrophotometer. In that way,

the data can be compared for the presence of the listed metal ions in the baking soda sample.

The first of the two methods being used to analyze the percent composition of sodium

bicarbonate in the baking soda will be via titration. In this case, the reaction used to figure out

the amount of sodium bicarbonate in the unknown baking soda sample will be

N aHCO 3 (s) + H Cl (aq) N aCl (aq) + H 2 O (l) + C O 2(g) . U

sing this chemical equation, one can

figure out the moles of sodium carbonate using

mol HCl mol N aHCO 3

L HCl used L HCl
mol HCl
= mol N aHCO 3 . Lastly, one can then calculate the percent

mass of sodium bicarbonate in the baking soda sample using the equation
84.01 g N aHCO 3 1
mol N aHCO 3 mol N aHCO 3
g Baking Soda
100% + percent mass N aHCO 3 . But before

performing the titrations to figure out the percent mass of sodium bicarbonate in the baking soda,

the exact molarity of the hydrochloric acid must be standardized. To figure out the molarity of

the hydrochloric acid, it will be standardized with N aHCO 3 . The same chemical equation will

be used. With this equation, the equation

mol of N aHCO 3(s) mol HCl (aq) 1
g of N aHCO 3(s) 84.01 g N aHCO 3(s)
mol N aHCO 3(s)
volume in L of HCl (aq) used @ equivalence point
= M HCl (aq)

can be derived stoichiometrically. The volume of H Cl at the first equivalent point for the

standardizations will be the one used for further calculations. During both the titrations, the

volume per drop of titrant needs to be figured out in order to convert the number of drops at the

equivalence point to milliliters. This can be done by taking the total volume used in each
titration and dividing it by the number drops used during the titrations. The data can then be

converted to read Volume v. pH instead of # drops v. pH using the ratio.

The second method that will be used to determine the mass percent of sodium

bicarbonate in the unknown baking soda sample will be via thermal gravimetric analysis. The

baking soda will be heated until sodium bicarbonate decomposes into gaseous water and carbon

dioxide. The amount of mass lost in the mixture through heating is the mass of water and carbon

dioxide that escaped the mixture. This mass is stoichiometrically related to the amount of

sodium bicarbonate in the mixture when looking at the molecular equation

2 N aHCO 3(s) N a 2 CO 3(s) + H 2 O (g) + C O 2(g) . From knowing the mass lost, the mass of

sodium bicarbonate in the mixture can be figured out. Using stoichiometry, we figure out that

for every two grams of N aHCO 3(s) , 0.107 grams of water and 0.262 grams of carbon dioxide

are lost. This means that for each gram of N aHCO 3(s) , 0.369 grams are lost. From there, the

mass of NaHCO3 can be calculated using the equation

2.00 g N aHCO 3
g lost ( 0.369 g lost
) = g N aHCO 3 initial sample . Then, the mass of NaHCO3 can be divided

by the total mass to figure out the percent mass composition using the equation
g N aHCO 3
g of Baking Soda
100% = percent mass N aHCO 3 .

Experimental

Reagents

1. Sodium bicarbonate (solid, primary standard base)

2. Baking soda sample (mixture)

 3. Approximately 1.0 M hydrochloric acid solution

4. 0.1 M Calcium chloride solution

5. 0.1 M Potassium chloride solution

6. 0.1 M Lithium chloride solution

Equipment

1. MeasureNet spectrophotometer and nichrome wires

2. MeasureNet pH probe and drop counter

3. Buret

4. Beral pipets

5. Kimwipes

6. Crucible and lid

7. Watch glass

8. 500 mL Beaker

Safety Precautions

Be sure to wear gloves at all times

Be sure to have safety goggles on at all times

Be wary of the hydrochloric acid

Setup
Solution Preparation

Emission Solutions

Pour the standard 0.1 M group IA and IIA metal chloride solutions into separate watch

glasses. To prepare the baking soda, take a good amount and dissolve it in water.

Titration Solutions

To prepare the baking soda or the sodium carbonate, take a good amount and dissolve it

in water in a 500 mL beaker using a magnetic stir bar and stir plate before their respective

titrations. Make sure the mass of baking soda or sodium carbonate used is recorded.

Part 1: Emission Spectroscopy

First, rinse the nichrome wire in distilled water to get rid of contaminants. Second, heat

up the wire. When the wire starts to glow a bright orange, position a watch glass with distilled

water near the air intake hole of the burner and place the wire into the distilled water. This

makes it so that the distilled water can spatter into the burner and clean the contaminants.
 Then with each of the metal chloride solutions and the baking soda solution, do the same

thing: heat up an uncontaminated piece of nichrome wire until it glows a bright orange, position

a watch glass with the respective metal chloride solution near the air intake hole of the burner

and place the wire into the solution to spatter. During each metal chloride solution test, press

Sample at the spectrophotometer to record the data. In addition, in between each metal chloride

solution, spatter the burner with distilled water to get rid of contaminants.

When recording, make sure the MeasureNet System is plotting the data (see if the graph

peaks). You should have the emission spectra for each metal chloride solution and the baking

soda.

Part 2: Titrations

Setup the MeasureNet drop counter, pH electrode, and buret assembly as well as the

MeasureNet System to create a pH v. Volume graph. Make sure you have rinsed the buret with

water and H Cl solution and have calibrated the pH electrode. Then, place the pH probe (with

the drop counter as support) in the beaker containing the N a 2 CO 3(s) . The tip of the probe must

be submerged. Make sure a stir bar is in the solution over a stir plate and that the N a 2 CO 3(s) is

completely dissolved. The stir bar must not touch the probe. Position the buret filled with H Cl

over the beaker and center it over the eye of the drop counter (will flash red with every drop).

Enter the initial volume of H Cl and start the titration by opening the buret valve so that H Cl is

added drop by drop. Make sure the stir bar continues stirring. When the titration is done, repeat

the process with another beaker of N a 2 CO 3(s) solution and with two trials of baking soda

solution. Lastly, do the necessary calculations.

Part 3: Thermal Gravimetric Analysis

For each crucible and lid, measure the mass and report it. Then add a good amount of

unknown baking soda to each crucible and measure the crucible and lid with the baking soda. In

this way, you can subtract the respective masses to find the mass of the baking soda. Place both

crucibles with their lids on a hot plate at 225-degrees-Celsius. Make sure the lids are placed

slightly ajar so that the water and carbon dioxide can escape. Wait for 10-15 minutes. Take the

tongs and remove the crucibles from the hot plate and place them on a mesh cooler. Weigh the

crucible, lid, and baking soda again. Repeat the process until the mass stays fairly constant

(0.001 off) for both crucibles. Lastly, do the necessary calculations.

Data Analysis

For the emission portion of the lab, first open all the files saved from the experiment in

Excel. Create a smooth lined scatter plot with the emission data from the baking soda sample

and group IA and IIA metal chloride solutions (wavelength v. intensity). Then, compare the line

for the baking soda sample with all the others to see which metals are present in the sample (the

metal is present if the graphs peak at the same wavelength).

For the titration portion of the lab, create separate smooth lined scatter plot for each of

the titration curves on Excel. Then, locate the equivalence points necessary for each titration and

report the number of drops at the equivalence points and the number of drops used throughout

each titration. Perform the necessary calculations.

Results

Unknown #823

PART 1: Emission Spectroscopy

Solution at Two Highest Intensities Color Present in Sample

(yes/no)

Baking Soda 588.98 (sodium), 766.23, 769.97 Orange

KCl 766.44, 770.15 Lilac Yes

LiCl 671.39 Magenta No

CaCl2 555.15, 624.90 Orange No

PART 2A: Standardization Trial #1 Trial #2

of HCl via Titration

Mass of NaHCO3 (g) 1.533 1.535

Initial Volume HCl soln 43.85 44.49

(mL)

Final Volume HCl soln 25.11 22.70

(mL(

Volume of HCl soln used 18.74 21.79

(mL)

# Drops Used 316 376

Volume per Drop (mL) 0.05930 0.05795

Volume of HCl soln used @ 13.503 13.581

Equivalence point (mL)

Molarity (M) HCl 0.9737 0.8385

Average Molarity HCl (M) 0.9062

Standardization HCl Trial #1 Calculations

Standardization HCl Trial #2 Calculations

PART 2B: Titration Trial #1 Trial #2

Mass Baking Soda (g) 1.001 1.014

Initial Volume HCl soln (mL) 44.11 43.86

Final Volume HCl soln (mL) 33.99 32.77

Volume of HCl soln used (mL) 10.12 11.09

# Drops Used 170 168

Volume per Drop (mL) 0.05953 0.06601

Volume of HCl soln used @ Equivalence point 3.750 3.917

(mL)

Percent Mass NaHCO3 (%) 28.1% 29.4%

Average Percent Mass NaHCO3 (%) 28.8%

Titration Trial #1 Calculations

Titration Trial #2 Calculations

PART 3: Thermal Gravimetric Analysis First Trial Second Trial

Mass of cool crucible & lid (g) 17.551 20.143

Mass of Baking Soda & cool crucible & lid 18.020 20.666

(g)

Mass of Baking Soda (g) 0.469 0.523

 Mass after 1st heating (g) 17.995 20.603

Mass after 2nd heating (g) 17.998 20.605

Mass after 3rd heating (g) N/A N/A

Mass of H20 and CO2 Lost (g) 0.0250 0.0630

Percent Mass NaHCO3 (%) 28.9 65.3 (OMIT)

Thermal Gravimetric Analysis Trial #1 Calculations

Thermal Gravimetric Analysis Trial #2 Calculations

 From the emission spectroscopy portion of the lab, it was found that only potassium was

present. From the titration portion of the lab, it was found that the percent mass of sodium

bicarbonate in the baking soda sample was 28.1-percent and 29.4-percent in the first and second

trials respectively with an average percent mass of 28.8-percent. From the thermal gravimetric

portion of the lab, it was found from the first trial that the percent mass was 28.9-percent. In the

second trial, it was found to be 65.3-percent, which was omitted.

Discussion

The results from the experiment were rather clear. The average percent mass of sodium

bicarbonate in the baking soda found via titration was extremely close to the percent mass found

in the first trial of the thermal gravimetric analysis as they were 28.8-percent and 28.9 percent

respectively (only 0.1-percent off). With the emission spectroscopy portion of the lab, it was

obvious both qualitatively and quantitatively that only potassium was present as a contaminant as

the sample had the same maximum intensity wavelengths as the potassium disregarding that of

sodium, which was given that it would be present; the sample had maximum intensity

wavelengths of 766.23 and 769.97 nanometers while potassium had maximum intensity

wavelengths of 766.44 and 770.15 nanometers.

While the results were clear for the first trial of the thermal gravimetric analysis, the

results for the second trial was an obvious outlier with a percent mass of 65.3-percent. Because

the results for the percent mass for the titrations and the first trial were so close, this 65.3-percent

was omitted. The large difference could be due to misreporting the mass of the cool crucible and
lid for the second trial, which was reported to be 20.143 grams. For example, if the mass had

been one less with 19.143 grams, the percent mass would have been calculated to be

22.4-percent, a result much closer in range to the others. With the titrations, it can be seen that

the pH would go back up and down, creating a rougher looking graph. This made it harder to

figure out the position of the equivalence point. Another possible source of error with the

titrations was that the drop counter did not sense a few drops during some trials. If the

experiment would to be improved, one way of doing so would be to use a more accurate and

precise pH probe. Another way would be to position the drop counter and buret in a way that the

drop counter will count every drop.

Conclusion

The purpose of this experiment was to analyze the composition of an unknown sample of

baking soda. To do so, titrations and thermal gravimetric analysis were used to figure out the

percent mass of sodium bicarbonate in the unknown sample. Emission spectroscopy was also

used to figure out which contaminants out of lithium, potassium, and calcium were present in the

sample. Via titration, it was found that the unknown sample, unknown #823, had a percent-mass

of sodium bicarbonate of 28.8-percent. Via thermal gravimetric analysis, it was found that the

percent mass of sodium bicarbonate was 28.9-percent. Lastly, via emission spectroscopy, it was

found that the unknown sample contained traces of potassium.

 Bibliography

Stanton, B., Zhu, L., & Atwood, C. H. (2006). Experiments in general chemistry featuring

MeasureNet. Belmont, CA: Thomson Brooks/Cole.

The book also provided the information needed for the procedure and detailed instructions. The

book also gave information on the theories behind spectroscopy, titrations, and thermal

gravimetric analysis.

Graybeal, J. D., Hurst, G. S., Stoner, J. O., & Chu, S. (2016, May 17). Spectroscopy - Theory of

molecular spectra. Retrieved November 08, 2016, from

https://www.britannica.com/science/spectroscopy/Theory-of-molecular-spectra. This site

offered more information on emission spectroscopy.